SU1145288A1 - Stationary phase for gas chromatography - Google Patents

Abstract

The use of S, K-diethylammonium salt of R-hpriphenyltrichloromethylphosphinic acid as a stationary phase for gas chromatography.

Description

The invention relates to the study of the chemical and physical properties of substances and concerns the gas chromatographic separation of mixtures of organic substances.

This phase can be found in the development of methods for the analysis of various chemical mixtures.

It is known the use of alkyl (arsH1) phosphonic acid esters as | {iod 1Znogo phase for gas chromatography | tj.

: The disadvantage of this phase is its thermal stability and insufficiently high selectivity of the separation of aromatic hydrocarbons from alcohols, ketones and nitro compounds.

It is known the use of tertiary oxide nitrile groups as a stationary phase for gas chromatography: The disadvantage of this phase is: in the high selectivity of separation of arbmatic hydrocarbons, ketoic alcohols and nitro compounds.

The purpose of the invention is to create a stationary phase with a high selectivity for the separation of aromatic hydrocarbons, alcohols, ketones and nitro compounds.

The delivered chain is achieved by using the H, H-Diethylammonium salt of IChlorfeiiptrichloromethylphosphine acid B as the stationary phase; for gas chromatography.

Previously, these compounds were not used as the stationary phase.

The direction of H, H-diethylamine copium l-chlorophenyltrichloromethyl phosphate acid is known as a reagent for organic synthesis {Z.

The sufficiency of the invention is T (km, that H, H-dynethylamine salt-chlorfexaIlPltrichlsflumethylphosphinic acid is applied on an inert or aTT & 8H solid carrier in an amount of 20-30% by weight and the sorbent thus obtained after the corresponding termination gas chromatographic separation of mixtures of organic substances is used.

The condition of the column is: 2000 mm column length, 3 mm diameter, analysis temperature, carrier gas rate (gels) 20/30 ml / min. Under these conditions, the retention times of the reference sorbents are determined and linear analogs of the field factors are calculated on their basis. rnness.

The separation selectivity is assessed on the basis of linear analogs of the polarity factors and their differences (X is benzene, methyl ethyl ketone, Y is ethanol, (J is nitromethane, 5 is pyridine).

The results obtained are compared with the results of the substances of analogues and the base 4 object (tricresyl phosphate). The results of the comparison are shown in the table.

The data in the table show that the stationary phase based on L, L-diethylammonium salt of p-phenyltrichloromethylphosphinic acid is characterized by high linear analogs of polarity factors: high polarity factor for reference sorbate methyl ethyl ketone (Z), and low polarity factor for benzene (X) . For a given substance, the difference between these polarity factors (Z-X) is greater than that of the base object and its analogues. So, this substance has a difference of Z - X 7.05 units. The corresponding difference in the polarity factors of the base object is 2 -X 1.84 units. To estimate the extreme selectivity of this stationary phase, a plot of the polarity 2 factors on X is plotted, which is shown in FIG. one.

From FIG. 1 that the point 1 corresponding to this stationary phase goes beyond the contour limiting the extreme values of the known range of stationary liquid phases. With respect to the base object (point 2) and analogous substances (points 3 and 4) for this fixed liquid phase, a significant shift of the extreme point is observed.

The table shows linear analogs of the fixed polarity factors.

phases at. I

The test was performed on an LHM-8VD chromatograph with a thermal conductivity detector. The separation temperature is 100-120 ° C; the carrier gas velocity is 30-40 ml / min; the column length is 2500 mm; helium is used as the carrier gas. The sorbent, prepared on the basis of the N, N-diethylammonium salt Ichlorophenyltrichloromethylphosphinic acid, is applied on a carrier of the Tsvetokhrom brand in the amount of 20-25% by weight

Jt1 "2884

carrier, followed by 4. chemilketone, methylpropyl ketone. Figure 2

the prepared column is provided with a separation chromatogram

IB thermostat chromatograph. Then in this mixture using a column,

a prepared chromatographic column of which, as a fixed phase, is introduced with different composition and projections used by KH-Diethylammonium.

The organic content of the mixture is p-chlorfenstrytrichloromethylphosphino (and benzene, toluene, xylene, methyl acid.

/

; H, M-diethylammonium

salt ft-chlorophenyltrichloromethylphosphine

 trunnnvu

Trncresyl phosphate (base object) (CH.) P-O

Diphenyl sfir cyclohex en-1-ylphosphonic acid (analog)

CH, -CH, -SY

/ " () R

About CHj-CH-CN

sn

0.5 8.56 7.55 7.35 5.08

1.743.22 2.58 4.14 2.95

1,785.73 3.57 3.85 2.42

4.14 8.42 5.85 6.06 7.10

.one

eight

7

2 6

1 G / i f ir S at 765 fPui.2 3 2 r 0

Claims (1)

The use of N, Ν-diethylammonium salt of P-chlorophenyltrichloromethylphosphinic acid as a stationary phase for gas chromatography. < The invention relates to studies of the chemical and physical properties of j. substances and for gas chromatographic separation of mixtures of organic substances. 5 This stationary phase can be used in the development of gas chromatographic analysis of various organic mixtures. It is known to use alkyl- ¹⁰ (aryl) phosphonic kirlot esters as the stationary phase for flj gas chromatography.